Resin-wax composition



Patented Sept. 13, 1949 UNITED STATES PATENT OFFICE 2.482.070 RESINJVAX COMPOSITION Daniel Schoenholz. Bronx, and Leon Brooklyn.

on to Inc., a corporation of New York No Drawing. Application June Foster D. S all:

801111 No. 679.585 7 chime. (CL 280-22) carnauba wax is expensive, it is generally extended with other waxes inclu those mentioned phenolics. certain other phenolics, and heat treated congo and enhancing certain desirable performance properties.

from dirt, uniformity of behavior, and wide m patibility, in a single mate ial.

We have now discovered that certain salts of a special type of resin are compatible with carnauba wax. other waxes, and resins hereinperslon of the mixture in medium.

Using our composition, we find it is possible to resin content a glossy film without the necessity These dispersions may have oleate are examples. resin solutions such as solutions may be used for the purpose oi obtainin various modifications or properties.

In one embodiment the invention comprises an organic emulsifying agent, to described.

Ahietic acid may be written as follows:

ups represented by can contain eon- The gro jugated double bonds. Although it is to this film. we esterify hydric alcohol. with the part of th erally by the following formula showing the proportion of the several radicals or groups:

I'OOC (CI-Ia) 2CH(CH:|) acid-I102 (32H: (CODE) 2 In this formula 1 represents an equivalent weight of the radical or residue of a polyhydric alcohol as. /2 mol of ethylene glycol less the hydroxyl groups, mol of glycerine less the hydroxyl groups, or mol of pentaerythritol less the hydroxyl groups.

The composition of the plex with glycerine may be lows:

maleic anhydride comrepresented as lol- CH: COOI' r in this instance represents V3 Cal-I5, that is, the equivalent weight of the glyceryl radical. Expressed difierently, the formula for a whole molecule would be CaHsXa, X representing all or the immediately preceding formula except the r.

When the complex represented by the above formula comes into contact with a warm aqueous solution of an alkali such as an amine (R.NH2), the anhydrlde groups on the right side of the formula given above are converted to salts, by a reaction which may be represented as follows:

As the alkali used to neutralize the acidity represented by the anhydride, or by the acid COOH groups after contact with water, there is used one that is water soluble. Particularly satisfactory results are obtained when the alkali is a soluble amine. Examples are a lower alkylamine, as, for instance. methyl, ethyl, or propylamine; an alkylolamine of which good examples are the mono-, di-, or triethanolamine, diethylethanolamine. and z-methyl Z-amino propanol. Another nitrogenous base that may be used is ammonia, although ammonia and alkali metal hydroxide, which may also be used as the alkali, are not as satisfactory as are the amines.

The wax to be used should be one that is conventionaliy used in polishing compositions of the class for which the present composition is to be used as a replacement. For convenience such 7 to the finished emulsion.

wax may be called a polishing wax, which means that, when properly compounded and applied as a thin film, in conventional manner, it gives a polish. The wax should be of satisfactory color, ordinarily light in color, non-tacky, and stable on exposure to air. Carnauba wax is the preferred example. Other waxes that may be used are candelilla, ouricuri, oxidized petroleum wax, microcrystalline petroleum wax, and macrocrystalline petroleum wax, either alone or mixed with each other or with carnauba. These waxes are known to be insoluble in water For a description of ouricuri emulsions in water, see U. S. Patent 2,383,451, issued to Cothran.

Examples of polyhydric alcohol that may be used are the di-, tri-, or tetrahydric alcohols, as, for instance, ethylene glycol, diethylene glycol, propylene glycol, glycerine, and pentaerythritol. When a composition that dries to give a bright film without polishing is not required, a monohydric alcohol may be used. Thus ior such use of the emulsion, r in the formula above may be methyl, ethyl, or butyl.

The abietic acid which is used in making the abietate oi the polyhydric alcohol may be substantially pure abietic acid but for economical commercial operations should be rosin or the resin acids fraction of tall oil.

The proportion of maleic anhydride to the abietate such as ester gum is suitably about 5 to 32 parts for 100 parts of the abietate. Best results are obtained within the range 9 to 30 parts,

or the salt of a maleic anhydride complex of the abietate of polyhydric alcohol we use up to the amount found by test to be compatible with the wax. When the salt used is the amine salt, there may be used as much as parts or slightly more of the salt to parts total weight of the salt and wax. Even in such large proportion, the amine salts are compatible with the wax, there is no instability of the dispersion in water, and no separation from the wax in the finished polishing film after evaporation of the water serving initially as the dispersion medium. For best results. we use about 20 to 45 parts of the salt to 100 of total weight of the salt and wax.

In general the dispersion of the present invention is made as follows:

The wax and the salt of the complex or ad junct of maleic acid with ester gum or like abietate of a polyhydric alcohol are warmed to a temperature above the melting point and stirred into water containing an organic alkali and also an emulsifying agent. If desired the wax and maleic acid complex from which the salt is to be made may be first melted together. In fact it is convenient, in commercial use of the invention, to melt together the wax and the maleicized ester gum or the like and then allow the mixture to solidify in containers for distribution, the solidified mass being remelted at the time of mixing into the aqueous dispersion medium.

As the emulsifying agent used in making the emulsion, a soap is preferred. Suitable examples are an alkali metal or an amine soap of a higher fatty acid, the oleates being particularly satisfactory. Other emulsiiying agents may be used, as, for instance, salts of the sulfated alcohols, other synthetic emulsifying agents such as the mannitan and sorbltan palmitate, and a polyglycol monooleate.

If a solution of an additional film forming ingradient is to be used it may be incorporated at the time of forming the emulsion or by addition Such film forming inassacro 8 gradient should be alkali :loluble, that is. diapcrsiham- 2 e in aqueous alkali solu on. Examp es of such ngredients that are satisfactory are shellac. case- W m m in, and the fusion product of main and rosin. The leiciz eater sum made as described in In place of the organic alkali used in forming g kamplc i was then melted with various resins the salts of the maleicized abietate of the pclyand waxes to give compositions of percentages by hydrlc alcohol, there may be used an inorganic we ht shown t following table;

alkali, as. for instance, sodium carbonate. potas- Each of the above blends, when melted and slum hydroxide. or borax. Much better results stirred with the dispersion medium including organic alkalies is not recommended except that dispersion in which the blend is the dispersed borax inircgizjunction with an organic alkali is phase Furthermore. the dispersion when apes e.

very d a plied and allowed to dry upon linoleum, sealed In any case the pH of the final composition wood, terrazzo pavement, or asphalt or rubber should not be much above so as to prevent tile, dries with a high lustre.

deteriorating effect of the composition on conventional flooring to which it may be applied and 3 also to avoid objectionable redispersibility ot the Preparation of dispersion film k1 Water- One hundred s Of an wax resi len h bright drying dispersions 0f the Present at as shown in the glgle of simple a 1 s zneize d fir invention are adapted for use also in other indusa steam jacketed kettle provided with a mechanitrles than floor waxe as, f r inflame, 511% cal agitator. The blend is warmed to and mainpollshes in w i h c se suita le dye or pigm tained at a temperature 01' 200-210 F. and there is in orp ra e as 11 towns material for is stirred in 7.5 parts Of 0161c acid and 9 parts of and alsoasa wax coating f r fruit& 4 triethanolamine. The oleic acid and a part of there may be used various proportions of none volatile material to water in the dispersion finally g g gg z g zzfig i 2:5,; 2? ze ggz z gf applied to the floor. A suitable proportion is 16 ethanolamme m 6 gallons or water at to 2100 o 30 parts of non-volatile materials to 100 parts amine along with the excess over the owe the other hand, the proportion of non-volatile c1 t materials should be increased to the amount reg i i i gg igfiz fi zg g g gg fg fi quire! give suitably thick mating in a single kettle. The whole is then stirred at 200 to 210 application. F t

The invention will be further illustrated by defi g i il gg gfi gfg gigg gg g igz g tailed description in connection with the followslowly with vigorous sfiiflng so as to insure unb ing'specitlc examples or steps in the practice of it. form incorporation into the batch as the water Exams: 1 is added and the water being added in the amount i I of 900 parts by weight. This gives an emulsion Mak no ma ei-cized resin containing approximately 12% of solids.

Commercial glyceryl abletate of the grade known as ester gum was used as the abietate of the polyhydric alcohol. This ester sum had a 80 In place or the ester gum used in Example 1 softening point by the ball and ring method or there is substituted an equal proportion of the 140 to 160 F., acid number 6 to 8. and saponiflsubstantially neutral ester of ethylene glycol with and held at a temperature of 320 to 355 F. until cedure of Example 1 is then followed and the foaming due to the expulsion of air and water product ohtalnedissubstituted on an equal weight had subsided. basis in the procedures of Examples 2 and 3.

For each 32 parts by weight of the remaining product there was admixed 3 parts of technical 5 maleic anhydride. Heating was continued and The procedure of Example 3 is followed except the resulting mixture held at a temperature of that the triethanolamine used therein is substi- 320" to 356 F. until foaming ceased. This retuted by an equivalent weight of any of the other quired 10 to 15 minutes. organic alkalies disclosed above.

The product was maleicized ester sum. It had a ball and ring softening point oi 213 m, an acid 6 value 01' 25 to 40, and saponiilcatlon value 175. There is made a warm melted blend at 200 to aisaoro 210' I. of the iollowins insredients, all proportion! being shown as parts by weight.

Parts water at 200 to cold water at 210 F. and then tap temperature.

in 380 parts oi.

300 parts of mam- 8 The addition of borax. which is particularly helpful in improving the qualities oi the emulsion which is to dry to a bright finish without bumne. is illustrated in this example.

As the wax resin blend there was selected any one those listed in the columns 1-10 in the table above.

of the selected wax resin blend was melted in a jacketed kettle provided with a methe temperature raised to 200 and 9 parts Then there was added a solution 01 7.5 parts parts of water at 200 to 210 F. stirred until the solution was thoroughly incorporated into the batch.

introduced sufficient additional parts of water added, to the composition this water beins added at 200 to 210 F.. slowly and with vigorous agitation.

mtely 12% of non-volatile materials which remain behind when the surface and the water caused to Exams: 9

An emulsion that is satisfactory tor many purposes is prepared by usin lkali metal hydroxide as the alkali to neutralize the maleic anhydride adjunct of the glyceryl abietate. The

t example illustrates this use.

Part A was prepared by making a blend at 200-2l0 F. of the following materials:

Parts Glyeervl ester gum 2! Maleicized ester gum 32 Oxidized petroleum wax. 14 carnauba #3 N. 0. Re! 18 Into this blend at 200-210 nrst 8 parts of sodi sodium and at the the water being ad and departures from the spirit the inversion of phase which occurs durins the addition oi the water.

28 parts at maleicized ester gum. 24 ct ester sum. 20 of carnauba wax. and i2 oi oxidized petroleum wax were blended at 200 to 210 F.

Into this blend at the same temperature, there were introduced 6.25 parts of oleic acid.

Then there were introduced. at F.. 5 parts aqua ammonia (28% concentration) in 25 oi at F., 2.5 parts of aqua am- 350 of water, and finally. at

Erma: 11

Borax was used in place 0! part of the ammonia oi Example 10. by adding to the melted wax resin blend and fatty acids a solution of 6 pounds of borax and 25 pounds of water at 210 1*. The ammonia additions are limited to 2.5 parts at 150 F. and 1.5 parts of ammonia at 190 F.

proportions are essentially as described in Example 10.

made as described are much less wax, are conin their results. They give non-tacky films that are evidently homogeneous and develop a high gloss without the need of bum s or otherwise polishing the film aiter the evaporation of the volatile dispersion medium.

stable, and give moderately alkaline solutions, as, i stance of pH 9 to 11 (or solutions 01 1% concentration of the salts.

It will be understood also to cover all changes and modifications oi the examples oi the invention herein chosen for the purpose of illustration which do not constitute and scope or the inventhat it is intended aim is:

1. An emulsion comprising a water-insoluble olishing wax, a salt of a water soluble nitrogenous alkali with the maleic anhydride adjunct oi the abietate oi. a polyhydric alcohol. water, and an emulsifying agent dissolved in the water. the the said salt being soluble in each other and being present in the emulsion as the dispersed phase and the salt being in the proportion of 20 to '15 parts to 100 parts of the salt and wax.

2. An emulsion comprising a water-insoluble polishing wax, a salt of a water soluble nitrogenous amine with the maleic anhydride adjunct of the abietate oi an aliphatic alcohol, water. and an emulsifying agent dissolved in the water and serving to improve the fineness of dispersion oi the wax and said salt. the wax and the said salt being soluble in each other and being present in the emulsion as the dispersed phase and the in the ro ortion of 20 to '75 parts to solved in the water.

for a polish, the composition comprisin a waterinsoluble polishing wax and a. salt 01' a water soluble nitrogenous alkali with the maleio anhydride adjunct of the abietate of a polyhydric alcohol and the proportion of the said salt being 20 to 75 parts for 100 parts of the salt and wax.

5. A composition suitable for use as the base for a polish, the

wax.

8. A composition for a. polish, the composition comprising carnauba ous solution of salt of a water DANIEL SCHOENHOLZ. LEON KRESSER.

REFERENCES CITED The following references are of record in the file of this potent: 

